CEM Phoenix Manuale utente

Operation ManualOperation Manual

Operation Manual

Innovators in

Microwave Technology

600134

Rev. 12

Phoenix™ and

Phoenix AirWave™

Microwave Furnace

This manual contains proprietary information

which shall not be disclosed or reproduced or transferred

to other documents without prior written permission

from CEM Corporation.

Phoenix is a trademark of CEM Corporation.

CEM is a registered trademark of CEM Corporation.

U.S. patents 5,066,834; 5,252,274;

5,318,754; 5,378,878; 5,441,681; and 5,468,135

Other U.S. and foreign patents pending

CEM Corporation

Matthews, North Carolina 28106

(704) 821-7015 FAX: (704) 821-7894 e-mail: [email protected]

MANUFACTURED IN THE

UNITED STATES OFAMERICA

600134

Rev. 12

4/2013

CAUTION

DO NOT install the Phoenix inside a fume hood.

To avoid the possibility of a thermal overload, the Phoenix should not be

physically located inside a fume hood. Vapors should be vented into a fume

hood by means of the exhaust hose only.

Installation of the Phoenix inside a fume hood will void any written or

implied warranty from the manufacturer.

WARNING

The mufﬂe furnace included with this instrument contains ceramic ﬁber

material and high temperature cement coating.

• Possible carcinogen based on tests with laboratory animals.

• May be irritating to skin, eyes and respiratory tract.

• May be harmful if swallowed or inhaled.

• Cristobalite (crystalline silica) formed at high temperatures

(above 1600° F) can cause severe respiratory disease.

For further information, call (800) 726-3331 and request Material Safety

Data Sheet part number 600531.

III

Operating Precautions

Do not tamper with the safety interlocks. The Phoenix™ is equipped with three door

safety interlock switches which prevent the instrument from producing microwave

power if the door is open. Tampering with the safety interlocks may allow microwave

production when the door is open, which is very dangerous.

Do not place any object between the front of the microwave cavity and the door or

allow soil or cleaner residue to accumulate on sealing surfaces.

Do not operate the instrument if it is damaged. It is particularly important that the

instrument door close properly and that there is no damage to the door (bent), hinges

or latches (broken or loosened), or door sealing surfaces.

The instrument utilizes high voltages and microwave radiation. It should be adjusted

or repaired only by qualiﬁed service personnel trained in repair and maintenance of

high voltage and microwave power systems.

The possibility of instrument-induced electromagnetic interference (EMI) is minimal

if precautions outlined in this manual are followed. However, it is recommended

that the user post a sign warning pacemaker wearers that a microwave device is in

operation. Also, the instrument should not be placed close to any electrical device

susceptible to EMI. If the instrument is suspected of inducing EMI, the door and the

front of the cavity should be carefully inspected for damage. A microwave leakage

measurement should be performed as outlined in the Maintenance and Service sec-

tion of this manual. Leakage above the legal limit of 5 mW/cm2should be reported

to the CEM Service Department.

WARNING

Improper installation or use of the instrument grounding wire and/or

plug can result in electrical shock.

The Phoenix instrument must be grounded. In the event of an electrical short circuit,

grounding reduces the risk of electric shock by providing an escape wire for the

electric current. This instrument is equipped with a cord having a grounding wire

with a grounding plug. The plug must be plugged into a dedicated outlet that is

properly installed and grounded.

If grounding instructions are not completely understood or if doubt exists that the

instrument is properly grounded, consult a qualiﬁed electrician or service technician.

If it is necessary to use an extension cord, use only a 3-wire extension cord with

a 3-blade grounding plug that has a 3 -slot electrical receptacle. The marked rating

of the extension cord shall be equal to or greater than the electrical rating of the

instrument.

Warnings, Cautions and Notes

Warnings, cautions and notes are included throughout this manual and should be read

thoroughly and strictly followed.

WARNING - A warning is inserted for essential information used to emphasize

dangerous or hazardous conditions to the operation, cleaning and maintenance of the

instrument which may result in personal injury.

CAUTION - A caution is inserted for essential information used to emphasize

procedures which, if not strictly followed, may result in damage or destruction to the

instrument or improper instrument operation.

NOTE - A note is inserted for emphasis of procedures or conditions which may

otherwise be misin-terpreted or overlooked and to clarify possible confusing situa-

tions.

To the best of our knowledge, the information contained herein is accurate. However,

CEM Corporation cannot accept liability of any kind for the accuracy or complete-

ness of the information contained in this manual. The ﬁnal determination of the

suitability and proper use of the instrument described herein, the accuracy of the

information and data obtained from such use, and whether such use infringes any

patents or the legal safeguards of others are the sole responsibility of the user.

Table of Contents

Introduction............................................................................................................ 1

Installation.............................................................................................................. 2

Installation Site .................................................................................................... 2

Unpacking............................................................................................................ 3

Inspection............................................................................................................... 6

Instrument Description........................................................................................... 7

Keyboard.............................................................................................................. 7

Door Protection....................................................................................................12

Furnace Door Holder Installation ........................................................................12

Instrument Startup................................................................................................12

External Balance Installation ...............................................................................16

External Balance Setup........................................................................................16

Printer Installation................................................................................................17

Personal Computer Setup.....................................................................................17

Setup Menu ............................................................................................................19

Auto Start/Stop.....................................................................................................20

External Balance ..................................................................................................21

System Options ....................................................................................................21

Timers ................................................................................................................21

Set Clock............................................................................................................22

Screen Saver Time .............................................................................................22

Tests ...................................................................................................................23

Information ........................................................................................................23

Controls..............................................................................................................24

Language............................................................................................................24

Password ............................................................................................................25

Program Options ................................................................................................ 25

Printer Setup.......................................................................................................26

Company Name .................................................................................................27

Delete Method....................................................................................................27

Quick Test - No External Balance..........................................................................29

Quick Test - External Balance ...............................................................................33

Standard ...............................................................................................................36

Syringe .................................................................................................................39

Edit/Create Method................................................................................................45

Create Method......................................................................................................45

Standard or Drying.............................................................................................46

Load Method..........................................................................................................49

Perform Method.....................................................................................................51

Standard or Drying Method - No External Balance.............................................51

Standard or Drying Method - External Balance ..................................................52

Standard .............................................................................................................54

Syringe ............................................................................................................... 58

Table of Contents (Continued)

Ramping Method - No External Balance.............................................................63

Ramping Method - External Balance (Standard).................................................65

Ramping Method - External Balance (Syringe)...................................................65

Print Menu .............................................................................................................79

Maintenance, Troubleshooting and Service...........................................................81

Routine Maintenance ...........................................................................................81

Microwave Leakage Measurement......................................................................83

Microwave Power Measurement .........................................................................84

Calibration............................................................................................................87

Furnace Temperature Calibration.......................................................................87

Enter Previous Calibration Values .....................................................................89

Troubleshooting Guide.........................................................................................90

Error Messages.....................................................................................................92

Component Removal and/or Replacement ..........................................................94

Fuses ..................................................................................................................94

Instrument Cover ...............................................................................................94

Furnace Thermocouple ......................................................................................97

Spare Parts ...........................................................................................................98

Speciﬁcations .........................................................................................................99

Warranty................................................................................................................101

Customer Support ...............................................................................................102

Options..................................................................................................................103

Sulfated Ash..........................................................................................................105

Introduction

The Microwave Mufﬂe Furnace, Model Phoenix, is a special purpose microwave

system designed for laboratory use in heating/ashing a wide range of materials. Its

primary purpose is the rapid oxidation of samples for the gravimetric determination

of ash content (loss on ignition).

Calculations for the Phoenix include

• % LOD (Loss on Drying) = Initial Weight-Final Weight (Dried Sample Weight)

x 100

• % Ash = Final Weight (Ash Weight)/Sample Weight x 100

• % ROI (Residue on Ignition) = Final Weight (Ash Weight)/Sample Weight)

x 100

• % LOI (Loss on Ignition) = Initial Weight - Final Weight (Ash Weight)/Sample

Weight) x 100

• % Total Residue = Final Weight (Dried)/Sample Weight x 100

• % Vol. Residue = Dried Weight – Ash Weight/Dried Weight x 100

• % Fixed Residue = Final Weight (Ashed)/Dried Weight x 100

The Phoenix system can be equipped with either a high temperature furnace or a

high capacity furnace. The high temperature furnace is for applications requiring

temperatures up to 1200 ºC. It can accommodate up to eight (8) CEM quartz ﬁber

crucibles. The high capacity furnace is for applications at or below 1000 ºC. It can

accommodate up to 15 CEM quartz ﬁber crucibles.

The Phoenix consists of

• a microwave power system.

• a stainless steel microwave cavity with exhaust fan,

• a programmable digital computer,

• a mufﬂe furnace, either high temperature or high capacity

• an internal temperature control system,

• internal calibration software,

• two (2) RS-232 ports and one (1) parallel printer port,

• exhaust hose to vent fumes, and

• furnace door holder.

Available accessories for use with the Phoenix include

• ashing crucibles and accessories,

• balances,

• printers, and

• calibration source instrumentation

Installation

The Phoenix instrument should be installed on a laboratory work bench with access

to a fume hood or other means of fume disposal.

Installation Site

To install the Phoenix, choose a location that:

1. provides at least 8 in. (20 cm) space on each side and 6 in. (15 cm) space in the

rear for proper ventilation.

2. is free from vibration of large equipment.

3. provides a temperature range of 41°F(5°C) to 104°F (40°C).

4. provides adequate bench space for sample handling and printer placement.

5. permits the instrument to be connected to a dedicated, grounded outlet. The

Phoenix instrument should be operated on a stabilized, constant voltage AC

power supply, and the voltage must be within ±10% of the speciﬁed level.

(Refer to the “Speciﬁcations” in this manual.)

Note: Measure line voltage to ensure that it meets system speciﬁcations.

CAUTION

Line voltage ﬂuctuations greater than 10% will affect instrument

performance.

6. provides access to a fume hood or other means of fume disposal.

CAUTION

Do not install the Phoenix instrument inside a fume hood. Placing

the instrument in a fume hood can cause a thermal overload. Vent

the Phoenix into a fume hood means of the exhaust hose.

7. (AirWave only) permits access to a compressed air supply (minimum 90 psi

@ 13 SCFM through a 1/4” to 5/16” ID air line with valve open and air ﬂowing

through system) (maximum 150 psi air pressure). If the Phoenix AirWave is

more than 50 feet from the compressed air supply, the air line should be

increased to 5/8” ID. Compressed air supply should be increased if the exhaust

hose is more than 16 feet. Air ﬂow is reduced by approximately 10% by each

additional 8-foot section of hose. The exhaust system is equipped with a male

quick disconnect coupler plug “M” style to be coupled with an “M” style female

coupler body (customer supplied).

8. (Phoenix Only) The exhaust system is designed to push fumes through the

exhaust hose (3” ID) at approximately 125 CFM (unducted). The exhaust system

will push fumes through the ﬂexible exhaust hose at approximately 55 - 75 Kmh

(40 - 55 mph). The exhaust hose should be a maximum length of 16 feet

(maximum 8 feet vertical within 16 feet).

WARNING

To avoid insufﬁcient exhaust, never permit the exhaust ﬂow rate to

fall below 50 CFM.

Unpacking

1. Carefully open the shipping cartons, using caution to avoid puncturing or

tearing the foam packaging. Remove the foam and cardboard packing material.

NOTE

Retain all packing material for use if returning the instrument to the

manufacturer for service.

2. With at least two people for lifting, locate the handles on each side of the

lifting carton and lift the instrument from the shipping carton and place it on a

laboratory bench. Carefully remove the lifting carton and plastic wrap from

the instrument.

3. Open the instrument door and remove the packing from the four studs in the

bottom of the instrument cavity.

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